CN106189209A - Polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds and preparation method thereof - Google Patents
Polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds and preparation method thereof Download PDFInfo
- Publication number
- CN106189209A CN106189209A CN201610723132.6A CN201610723132A CN106189209A CN 106189209 A CN106189209 A CN 106189209A CN 201610723132 A CN201610723132 A CN 201610723132A CN 106189209 A CN106189209 A CN 106189209A
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- CN
- China
- Prior art keywords
- polyamide
- organic black
- black masterbatch
- boron nitride
- heat conduction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- 229920002647 polyamide Polymers 0.000 title claims abstract description 96
- 239000004952 Polyamide Substances 0.000 title claims abstract description 95
- 239000004594 Masterbatch (MB) Substances 0.000 title claims abstract description 61
- 239000000463 material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 229910052582 BN Inorganic materials 0.000 claims abstract description 78
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims abstract description 78
- 229910052581 Si3N4 Inorganic materials 0.000 claims abstract description 59
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 59
- 239000000853 adhesive Substances 0.000 claims abstract description 55
- 230000001070 adhesive effect Effects 0.000 claims abstract description 55
- 239000002135 nanosheet Substances 0.000 claims abstract description 54
- -1 polypropylene Polymers 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 21
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000077 silane Inorganic materials 0.000 claims abstract description 18
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 17
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 17
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 16
- 239000004743 Polypropylene Substances 0.000 claims abstract description 16
- 239000004917 carbon fiber Substances 0.000 claims abstract description 16
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229920001155 polypropylene Polymers 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims description 22
- 239000006052 feed supplement Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 20
- 229920005989 resin Polymers 0.000 claims description 17
- 239000011347 resin Substances 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 13
- 229920006122 polyamide resin Polymers 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 6
- 229910052796 boron Inorganic materials 0.000 claims description 6
- 150000002148 esters Chemical class 0.000 claims description 4
- ILNDSSCEZZFNGE-UHFFFAOYSA-N 1,3-Di-tert-butylbenzene Chemical compound CC(C)(C)C1=CC=CC(C(C)(C)C)=C1 ILNDSSCEZZFNGE-UHFFFAOYSA-N 0.000 claims description 2
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000003508 Dilauryl thiodipropionate Substances 0.000 claims description 2
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical class CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 239000004840 adhesive resin Substances 0.000 claims description 2
- 229920006223 adhesive resin Polymers 0.000 claims description 2
- 235000019304 dilauryl thiodipropionate Nutrition 0.000 claims description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 2
- 239000001177 diphosphate Substances 0.000 claims description 2
- 235000011180 diphosphates Nutrition 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical group CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- MBGQQKKTDDNCSG-UHFFFAOYSA-N ethenyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(C=C)OCC MBGQQKKTDDNCSG-UHFFFAOYSA-N 0.000 claims description 2
- DUWWHGPELOTTOE-UHFFFAOYSA-N n-(5-chloro-2,4-dimethoxyphenyl)-3-oxobutanamide Chemical compound COC1=CC(OC)=C(NC(=O)CC(C)=O)C=C1Cl DUWWHGPELOTTOE-UHFFFAOYSA-N 0.000 claims description 2
- GLDOVTGHNKAZLK-UHFFFAOYSA-N n-octadecyl alcohol Natural products CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 2
- 150000008301 phosphite esters Chemical class 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 235000019260 propionic acid Nutrition 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 7
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 238000005453 pelletization Methods 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 238000004040 coloring Methods 0.000 description 3
- 239000011229 interlayer Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000945 filler Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000002783 friction material Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2310/00—Masterbatches
Abstract
The invention discloses the polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds, in parts by weight, including following components: polyamide 50 90 parts, boron nitride nanosheet 0.01 2 parts, boron nitride powder 59 parts, nano-silicon nitride 24 parts, Organic Black Masterbatch 36 parts, 6 11 parts of carbon fiber, 13 parts of maleic anhydride inoculated polypropylene wax, silane coupler 0.5 1.2 parts, adhesive 25 parts, 0.3 0.7 parts of antioxidant.The invention also discloses the preparation method of this high heat conduction polyamide compoiste material.The present invention is by adding boron nitride nanosheet and boron nitride powder in polyamide, additionally add nano-silicon nitride, independent heat conduction network is constituted between three, the composite heat conductivility prepared is improved, and the wearability of this composite, impact resistance are also greatly improved.
Description
Technical field:
The present invention relates to field of compound material, the polyamide being specifically related to the interpolation of a kind of high heat conduction Organic Black Masterbatch is multiple
Condensation material.
Background technology:
In recent years, pursuing miniaturization at electronic device, high frequency, light-weighted today, macromolecule thermal-conducting polymer is whereby
Becoming the rising star in Heat Conduction Material field, its application the most gradually extends, such as heat exchange engineering, electric, friction material, electromagnetism
Shielding, auto manufacturing etc..But it is the non-conductor of heat mostly due to polymers, the most under normal conditions, without any
The macromolecular material of process or modification usually can not undertake the task of heat sink material.High molecular thermal conductivity is relatively
Little, only by it is modified, its corresponding performance could be improved further, thus expand its application.Wherein, by
In polyamide, there is a lot of excellent performance, such as high tensile, high impact, superior heat resistance, excellent resistance toization
Learn corrosivity etc., paid close attention to by widely studied person.
At present, the method for the heat conductivility improving polyamide is mainly added appropriate in polyamide-based bottom resin
Heat filling, but when using the heat conductivity that the method improves polyamide material, it is generally required to add more filler, ability
Make its heat conductivility have the change of a matter, this not only adds production cost, and the addition of more filler is also to polyamide resin
The mechanical property of fat has a great impact.
Summary of the invention:
It is an object of the invention to provide the polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds, this composite wood
Material excellent thermal conductivity, wear-resisting, scratch resistance excellent performance, shock resistance is good.
It is a further object to provide the system of the polyamide compoiste material that this high heat conduction Organic Black Masterbatch adds
Preparation Method.
For achieving the above object, the present invention is by the following technical solutions:
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds, in parts by weight, including following components:
Polyamide 50-90 part, boron nitride nanosheet 0.01-2 part,
Boron nitride powder 5-9 part, nano-silicon nitride 2-4 part,
Organic Black Masterbatch 3-6 part, carbon fiber 6-11 part,
Maleic anhydride inoculated polypropylene wax 1-3 part, silane coupler 0.5-1.2 part,
Adhesive 2-5 part, antioxidant 0.3-0.7 part.
Preferred as technique scheme, the size of described nano-silicon nitride is 15-30nm.
Preferred as technique scheme, described Organic Black Masterbatch, by percentage to the quality, by following components group
Become:
Polyamide 50-70%,
Nigrosine toner 30-50%.
Preferred as technique scheme, described boron nitride nanosheet is to be peeled off legal system by boron nitride powder by solvent
, its thickness is 10-20nm, a diameter of 1-2 μm.
Preferred as technique scheme, described adhesive is polystyrene type adhesive, ethyl acetate class adhesive
Mixing, both mass ratioes are 1:(1.5-2.2).
Preferred as technique scheme, described silane coupler is VTES, vinyl front three
One or more mixing in TMOS, vinyl methyl diethoxy silane.
Preferred as technique scheme, described antioxidant is pentaerythrite diphosphate ester two (2,4-di-t-butylbenzenes
Base) ester, phosphite ester three (2,4-di-tert-butyl phenyl) ester, dilauryl thiodipropionate, β-(4-hydroxy phenyl-3,5-two
The tert-butyl group) one or more mixing in propanoic acid positive octadecanol ester.
Preferred as technique scheme, described polyamide is spherical or almost spherical.
The preparation method of the polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds, comprises the following steps:
(1) under normal temperature condition, boron nitride nanosheet, nano-silicon nitride are respectively classified into 2-4 equal portions, the most by several times
Join in adhesive, stir, be placed in Vltrasonic device, supersound process 30-50min under 600W, obtain boron nitride and receive
Rice sheet, nano-silicon nitride adhesive；
(2) polyamide is joined in the prepared boron nitride nanosheet of step (1), nano-silicon nitride adhesive, stir
Mix uniformly so that be mixed with boron nitride nanosheet, the adhesive of nano-silicon nitride is uniformly dispersed in polyamide surface, obtains
It is enclosed with boron nitride nanosheet, the resin of nano-silicon nitride adhesive；
(3) under normal temperature condition, boron nitride powder is divided into 2-3 equal portions, joins prepared being enclosed with of step (2) by several times
Boron nitride nanosheet, nano-silicon nitride adhesive resin in, be uniformly mixed, then at 50-80 DEG C be dried 15-30h,
Obtain modified polyamide resin；
(4) polyamide and the metering conveying of nigrosine toner, metering and conveying device comprises two independent feed supplement feed bins
With the weighing balance of two band feed hopper, polyamide and nigrosine toner are put into respective feed supplement feed bin, then leads to
Cross feed supplement feed bin and enter the feed hopper on respective weighing balance, be finally delivered in double screw extruder melt extrude pelletize, draw
Bar water-cooled pelletizing or underwater cutpellet, be dried 2-5h, obtain Organic Black Masterbatch at 80-120 DEG C after pelletize；
(5) modified polyamide resin step (3) prepared and step (4) add after preparing Organic Black Masterbatch mix homogeneously
Enter in high-speed mixer, in high-speed mixer, be then sequentially added into carbon fiber, maleic anhydride inoculated polypropylene wax, silane occasionally
Connection agent, antioxidant, mix 20-40min, obtain compound under the mixing speed of 700-800r/min；
(6) compound that step (5) prepares is joined in double screw extruder, melt extrude pelletize, after granulated and dried
Obtain the polyamide compoiste material that high heat conduction Organic Black Masterbatch adds.
Preferred as technique scheme, when step (4) melt extrudes pelletize, the screw rod of described double screw extruder
Each section and head temperature are respectively as follows: feeding section: 115-125 DEG C, 200-220 DEG C, transportation section, melt zone 230-245 DEG C, head
225-230℃。
Compared with prior art, the method have the advantages that
(1) present invention adds appropriate boron nitride nanosheet, boron nitride powder and nano-silicon nitride in base resin,
Preparing material outermost layer is boron nitride powder, and centre is resin, and intermediate layer is boron nitride nanosheet, nano-silicon nitride adhesive,
Nm-class boron nitride is dispersed in the interlayer of boron nitride nanosheet, and prepared modified resin dispersion is good, and stability is excellent, its outermost
The boron nitride powder of layer and the boron nitride nanosheet in intermediate layer, nano-silicon nitride can form independent passage of heat, its heat conduction
Performance is far longer than individually adds the heat-conducting effect that boron nitride, boron nitride nanosheet or nano-silicon nitride are brought, and very small amount
Boron nitride nanosheet, the interpolation of nano-silicon nitride just can be effectively improved the heat conductivity of polyamide, and nano-silicon nitride
Granule is dispersed in the interlayer of boron nitride nanosheet, increase distance between layers, it is to avoid the interlayer of boron nitride nanosheet
Reunite so that the heat conductivility of material is the most lasting；
(2) on the other hand, the present invention also adds organic black agglomerate in polyamide and also colours it, organic
Black agglomerate is nigrosine toner to be melt extruded pelletize with polyamide and prepares, the content of both conservative control of the present invention and
Preparation process condition so that prepared Organic Black Masterbatch is splendid with the compatibility of polyamide, and its photoextinction is weaker than charcoal
Black, after coloring resinous luster Du Genggao, coloring is the most evenly；
(3) when the present invention prepares Organic Black Masterbatch, using metering mode of movement conveying raw material, metering is accurate, therefore
The quality of the product obtained is sufficiently stable, also improves the uniformity of polyamide material coloring, and work flow is closed, and will not produce
Dust, it is ensured that the neat and tidy of working environment, decreases the harm to operator；
(4) present invention is also added with appropriate carbon fiber, maleic anhydride grafting in preparing high heat conduction polyamide compoiste material
Polypropylene wax, silane coupler, effectively improve the wear-resisting of base resin, scratch resistance performance, and its toughness also obtains effectively
Improve；The polyamide compoiste material good stability that the present invention prepares, preparation method is simple, low cost.
Detailed description of the invention:
In order to be better understood from the present invention, below by embodiment, the present invention is further described, and embodiment is served only for solving
Release the present invention, the present invention will not be constituted any restriction.
Embodiment 1
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds, in parts by weight, including following components:
Polyamide 50 parts, boron nitride nanosheet 0.01 part,
Boron nitride powder 5 parts, nano-silicon nitride 2 parts,
Organic Black Masterbatch 3 parts, 6 parts of carbon fiber,
1 part of maleic anhydride inoculated polypropylene wax, silane coupler 0.5 part,
Adhesive 2 parts, 0.3 part of antioxidant；
Organic Black Masterbatch, by percentage to the quality, including polyamide 50%, nigrosine toner 50%；
The preparation method of this composite comprises the following steps:
(1) under normal temperature condition, boron nitride nanosheet, nano-silicon nitride are respectively classified into 2 equal portions, add the most by several times
Enter in adhesive, stir, be placed in Vltrasonic device, supersound process 30min under 600W, obtain boron nitride nanosheet,
Nano-silicon nitride adhesive；
(2) polyamide is joined in the prepared boron nitride nanosheet of step (1), nano-silicon nitride adhesive, stir
Mix uniformly so that be mixed with boron nitride nanosheet, the adhesive of nano-silicon nitride is uniformly dispersed in polyamide surface, obtains
It is enclosed with boron nitride nanosheet, the resin of nano-silicon nitride adhesive；
(3) under normal temperature condition, boron nitride powder being divided into 2 equal portions, join that step (2) prepares by several times is enclosed with nitrogen
Change in the resin of boron nanometer sheet, nano-silicon nitride adhesive, be uniformly mixed, at 50 DEG C, be then dried 30h, obtain modification
Polyamide；
(4) polyamide and the metering conveying of nigrosine toner, metering and conveying device comprises two independent feed supplement feed bins
With the weighing balance of two band feed hopper, polyamide and nigrosine toner are put into respective feed supplement feed bin, then leads to
Cross feed supplement feed bin and enter the feed hopper on respective weighing balance, be finally delivered in double screw extruder melt extrude pelletize, draw
Bar water-cooled pelletizing or underwater cutpellet, be dried 5h, obtain Organic Black Masterbatch at 80 DEG C after pelletize, wherein, when melt extruding pelletize,
The screw zones of described double screw extruder and head temperature are respectively as follows: feeding section: 115 DEG C, 200 DEG C, transportation section, melt zone
230 DEG C, head 225 DEG C；
(5) modified polyamide resin step (3) prepared and step (4) add after preparing Organic Black Masterbatch mix homogeneously
Enter in high-speed mixer, in high-speed mixer, be then sequentially added into carbon fiber, maleic anhydride inoculated polypropylene wax, silane occasionally
Connection agent, antioxidant, mix 40min, obtain compound under the mixing speed of 700r/min；
(6) compound that step (5) prepares is joined in double screw extruder, melt extrude pelletize, after granulated and dried
Obtain the polyamide compoiste material that high heat conduction Organic Black Masterbatch adds.
Embodiment 2
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds, in parts by weight, including following components:
Polyamide 90 parts, boron nitride nanosheet 2 parts,
Boron nitride powder 9 parts, nano-silicon nitride 4 parts,
Organic Black Masterbatch 6 parts, 11 parts of carbon fiber,
3 parts of maleic anhydride inoculated polypropylene wax, silane coupler 1.2 parts,
Adhesive 5 parts, 0.7 part of antioxidant；
Organic Black Masterbatch, by percentage to the quality, including polyamide 70%, nigrosine toner 30%；
The preparation method of this composite comprises the following steps:
(1) under normal temperature condition, boron nitride nanosheet, nano-silicon nitride are respectively classified into 2 equal portions, add the most by several times
Enter in adhesive, stir, be placed in Vltrasonic device, supersound process 50min under 600W, obtain boron nitride nanosheet,
Nano-silicon nitride adhesive；
(2) polyamide is joined in the prepared boron nitride nanosheet of step (1), nano-silicon nitride adhesive, stir
Mix uniformly so that be mixed with boron nitride nanosheet, the adhesive of nano-silicon nitride is uniformly dispersed in polyamide surface, obtains
It is enclosed with boron nitride nanosheet, the resin of nano-silicon nitride adhesive；
(3) under normal temperature condition, boron nitride powder being divided into 2 equal portions, join that step (2) prepares by several times is enclosed with nitrogen
Change in the resin of boron nanometer sheet, nano-silicon nitride adhesive, be uniformly mixed, at 80 DEG C, be then dried 15h, obtain modification
Polyamide；
(4) polyamide and the metering conveying of nigrosine toner, metering and conveying device comprises two independent feed supplement feed bins
With the weighing balance of two band feed hopper, polyamide and nigrosine toner are put into respective feed supplement feed bin, then leads to
Cross feed supplement feed bin and enter the feed hopper on respective weighing balance, be finally delivered in double screw extruder melt extrude pelletize, draw
Bar water-cooled pelletizing or underwater cutpellet, be dried 2h, obtain Organic Black Masterbatch, wherein, melt extrude pelletize at 120 DEG C after pelletize
Time, the screw zones of described double screw extruder and head temperature be respectively as follows: feeding section: 125 DEG C, and 220 DEG C, transportation section is melted
Section 245 DEG C, head 230 DEG C；
(5) modified polyamide resin step (3) prepared and step (4) add after preparing Organic Black Masterbatch mix homogeneously
Enter in high-speed mixer, in high-speed mixer, be then sequentially added into carbon fiber, maleic anhydride inoculated polypropylene wax, silane occasionally
Connection agent, antioxidant, mix 20min, obtain compound under the mixing speed of 800r/min；
(6) compound that step (5) prepares is joined in double screw extruder, melt extrude pelletize, after granulated and dried
Obtain the polyamide compoiste material that high heat conduction Organic Black Masterbatch adds.
Embodiment 3
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds, in parts by weight, including following components:
Polyamide 60 parts, boron nitride nanosheet 0.50 part,
Boron nitride powder 6 parts, nano-silicon nitride 2.5 parts,
Organic Black Masterbatch 4 parts, 7 parts of carbon fiber,
1.5 parts of maleic anhydride inoculated polypropylene wax, silane coupler 0.7 part,
Adhesive 3 parts, 0.4 part of antioxidant；
Organic Black Masterbatch, by percentage to the quality, including polyamide 55%, nigrosine toner 45%；
The preparation method of this composite comprises the following steps:
(1) under normal temperature condition, boron nitride nanosheet, nano-silicon nitride are respectively classified into 3 equal portions, add the most by several times
Enter in adhesive, stir, be placed in Vltrasonic device, supersound process 35min under 600W, obtain boron nitride nanosheet,
Nano-silicon nitride adhesive；
(2) polyamide is joined in the prepared boron nitride nanosheet of step (1), nano-silicon nitride adhesive, stir
Mix uniformly so that be mixed with boron nitride nanosheet, the adhesive of nano-silicon nitride is uniformly dispersed in polyamide surface, obtains
It is enclosed with boron nitride nanosheet, the resin of nano-silicon nitride adhesive；
(3) under normal temperature condition, boron nitride powder being divided into 2 equal portions, join that step (2) prepares by several times is enclosed with nitrogen
Change in the resin of boron nanometer sheet, nano-silicon nitride adhesive, be uniformly mixed, at 60 DEG C, be then dried 20h, obtain modification
Polyamide；
(4) polyamide and the metering conveying of nigrosine toner, metering and conveying device comprises two independent feed supplement feed bins
With the weighing balance of two band feed hopper, polyamide and nigrosine toner are put into respective feed supplement feed bin, then leads to
Cross feed supplement feed bin and enter the feed hopper on respective weighing balance, be finally delivered in double screw extruder melt extrude pelletize, draw
Bar water-cooled pelletizing or underwater cutpellet, be dried 3h, obtain Organic Black Masterbatch at 90 DEG C after pelletize, wherein, when melt extruding pelletize,
The screw zones of described double screw extruder and head temperature are respectively as follows: feeding section: 117 DEG C, 205 DEG C, transportation section, melt zone
235 DEG C, head 225 DEG C；
(5) modified polyamide resin step (3) prepared and step (4) add after preparing Organic Black Masterbatch mix homogeneously
Enter in high-speed mixer, in high-speed mixer, be then sequentially added into carbon fiber, maleic anhydride inoculated polypropylene wax, silane occasionally
Connection agent, antioxidant, mix 25min, obtain compound under the mixing speed of 750r/min；
(6) compound that step (5) prepares is joined in double screw extruder, melt extrude pelletize, after granulated and dried
Obtain the polyamide compoiste material that high heat conduction Organic Black Masterbatch adds.
Embodiment 4
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds, in parts by weight, including following components:
Polyamide 70 parts, boron nitride nanosheet 1 part,
Boron nitride powder 7 parts, nano-silicon nitride 3 parts,
Organic Black Masterbatch 4.5 parts, 8 parts of carbon fiber,
2 parts of maleic anhydride inoculated polypropylene wax, silane coupler 0.9 part,
Adhesive 4 parts, 0.5 part of antioxidant；
Organic Black Masterbatch, by percentage to the quality, including polyamide 60%, nigrosine toner 40%；
The preparation method of this composite comprises the following steps:
(1) under normal temperature condition, boron nitride nanosheet, nano-silicon nitride are respectively classified into 3 equal portions, add the most by several times
Enter in adhesive, stir, be placed in Vltrasonic device, supersound process 40min under 600W, obtain boron nitride nanosheet,
Nano-silicon nitride adhesive；
(2) polyamide is joined in the prepared boron nitride nanosheet of step (1), nano-silicon nitride adhesive, stir
Mix uniformly so that be mixed with boron nitride nanosheet, the adhesive of nano-silicon nitride is uniformly dispersed in polyamide surface, obtains
It is enclosed with boron nitride nanosheet, the resin of nano-silicon nitride adhesive；
(3) under normal temperature condition, classify in three categories part by boron nitride powder, and join by several times that step (2) prepares is enclosed with nitrogen
Change in the resin of boron nanometer sheet, nano-silicon nitride adhesive, be uniformly mixed, at 70 DEG C, be then dried 22h, obtain modification
Polyamide；
(4) polyamide and the metering conveying of nigrosine toner, metering and conveying device comprises two independent feed supplement feed bins
With the weighing balance of two band feed hopper, polyamide and nigrosine toner are put into respective feed supplement feed bin, then leads to
Cross feed supplement feed bin and enter the feed hopper on respective weighing balance, be finally delivered in double screw extruder melt extrude pelletize, draw
Bar water-cooled pelletizing or underwater cutpellet, be dried 4h, obtain Organic Black Masterbatch, wherein, melt extrude pelletize at 100 DEG C after pelletize
Time, the screw zones of described double screw extruder and head temperature be respectively as follows: feeding section: 120 DEG C, and 210 DEG C, transportation section is melted
Section 240 DEG C, head 230 DEG C；
(5) modified polyamide resin step (3) prepared and step (4) add after preparing Organic Black Masterbatch mix homogeneously
Enter in high-speed mixer, in high-speed mixer, be then sequentially added into carbon fiber, maleic anhydride inoculated polypropylene wax, silane occasionally
Connection agent, antioxidant, mix 35min, obtain compound under the mixing speed of 700r/min；
(6) compound that step (5) prepares is joined in double screw extruder, melt extrude pelletize, after granulated and dried
Obtain the polyamide compoiste material that high heat conduction Organic Black Masterbatch adds.
Embodiment 5
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch adds, in parts by weight, including following components:
Polyamide 80 parts, boron nitride nanosheet 1.5 parts,
Boron nitride powder 8 parts, nano-silicon nitride 3.5 parts,
Organic Black Masterbatch 5 parts, 10 parts of carbon fiber,
2.5 parts of maleic anhydride inoculated polypropylene wax, silane coupler 1.1 parts,
Adhesive 4 parts, 0.6 part of antioxidant；
Organic Black Masterbatch, by percentage to the quality, including polyamide 65%, nigrosine toner 35%；
The preparation method of this composite comprises the following steps:
(1) under normal temperature condition, boron nitride nanosheet, nano-silicon nitride are respectively classified into 4 equal portions, add the most by several times
Enter in adhesive, stir, be placed in Vltrasonic device, supersound process 45min under 600W, obtain boron nitride nanosheet,
Nano-silicon nitride adhesive；
(2) polyamide is joined in the prepared boron nitride nanosheet of step (1), nano-silicon nitride adhesive, stir
Mix uniformly so that be mixed with boron nitride nanosheet, the adhesive of nano-silicon nitride is uniformly dispersed in polyamide surface, obtains
It is enclosed with boron nitride nanosheet, the resin of nano-silicon nitride adhesive；
(3) under normal temperature condition, classify in three categories part by boron nitride powder, and join by several times that step (2) prepares is enclosed with nitrogen
Change in the resin of boron nanometer sheet, nano-silicon nitride adhesive, be uniformly mixed, at 75 DEG C, be then dried 26h, obtain modification
Polyamide；
(4) polyamide and the metering conveying of nigrosine toner, metering and conveying device comprises two independent feed supplement feed bins
With the weighing balance of two band feed hopper, polyamide and nigrosine toner are put into respective feed supplement feed bin, then leads to
Cross feed supplement feed bin and enter the feed hopper on respective weighing balance, be finally delivered in double screw extruder melt extrude pelletize, draw
Bar water-cooled pelletizing or underwater cutpellet, be dried 4.5h, obtain Organic Black Masterbatch, wherein, melt extrude pelletize at 110 DEG C after pelletize
Time, the screw zones of described double screw extruder and head temperature be respectively as follows: feeding section: 125 DEG C, and 210 DEG C, transportation section is melted
Section 240 DEG C, head 228 DEG C；
(5) modified polyamide resin step (3) prepared and step (4) add after preparing Organic Black Masterbatch mix homogeneously
Enter in high-speed mixer, in high-speed mixer, be then sequentially added into carbon fiber, maleic anhydride inoculated polypropylene wax, silane occasionally
Connection agent, antioxidant, mix 25min, obtain compound under the mixing speed of 800r/min；
(6) compound that step (5) prepares is joined in double screw extruder, melt extrude pelletize, after granulated and dried
Obtain the polyamide compoiste material that high heat conduction Organic Black Masterbatch adds.
By the polyamide compoiste material pellet prepared by the present invention, carry out injection system by HTF200-w1 injection (mo(u)lding) machine
Sample, and prepared sample is carried out performance test.
(1) thermal conductivity test
The laser method heat transfer analysis instrument LFA457 using Nai Chi instrument manufacturing company limited of Germany to produce presses ASTM E1461
The thermal conductivity of the polyamide compoiste material prepared by mensuration, injection molding sample is diameter 12.5mm, and thickness is 2-2.5mm's
Disk.
(2) tensile property test
Sample tensile property uses WDW type microcomputer controlled electronic universal tester to study, according to GB/T
1040.2-1006 standard test.Experimental temperature is 25 DEG C, sets draw speed as 50mm/min.Edge on standard specimen
Axle applies tensile load.Until sample is pulled off, test, characterize the quality of material tensile property by hot strength.
(3) impact strength test
The impact strength of composite is according to using notched specimen simple beam impact strength method of testing mensuration, according to GB/T
1043-1993 tests.
Test result is as shown in table 1.
Table 1
From the point of view of table 1, the polyamide compoiste material that the present invention prepares has higher thermal conductivity, good heat conductivity, and power
Learn excellent performance.
Claims (10)
1. the polyamide compoiste material that one kind high heat conduction Organic Black Masterbatch adds, it is characterised in that in parts by weight, including with
Lower component:
Polyamide 50-90 part, boron nitride nanosheet 0.01-2 part,
Boron nitride powder 5-9 part, nano-silicon nitride 2-4 part,
Organic Black Masterbatch 3-6 part, carbon fiber 6-11 part,
Maleic anhydride inoculated polypropylene wax 1-3 part, silane coupler 0.5-1.2 part,
Adhesive 2-5 part, antioxidant 0.3-0.7 part.
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch the most as claimed in claim 1 adds, it is characterised in that
The size of described nano-silicon nitride is 15-30nm.
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch the most as claimed in claim 1 adds, it is characterised in that
Described Organic Black Masterbatch, by percentage to the quality, composed of the following components:
Polyamide 50-70%,
Nigrosine toner 30-50%.
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch the most as claimed in claim 1 adds, it is characterised in that
Described boron nitride nanosheet is to be prepared by solvent stripping method by boron nitride powder, and its thickness is 10-20nm, a diameter of 1-2 μm.
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch the most as claimed in claim 1 adds, it is characterised in that
Described adhesive is polystyrene type adhesive, the mixing of ethyl acetate class adhesive, and both mass ratioes are 1:(1.5-2.2).
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch the most as claimed in claim 1 adds, it is characterised in that
Described silane coupler is VTES, vinyltrimethoxy silane, vinyl methyl diethoxy silane
In one or more mixing.
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch the most as claimed in claim 1 adds, it is characterised in that
Described antioxidant is pentaerythrite diphosphate ester two (2,4-di-tert-butyl phenyl) ester, phosphite ester three (2,4-di-t-butylbenzene
Base) ester, dilauryl thiodipropionate, one in β-(4-hydroxy phenyl-3,5-di-t-butyl) propanoic acid positive octadecanol ester
Or several mixing.
The polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch the most as claimed in claim 1 adds, it is characterised in that
Described polyamide is spherical or almost spherical.
9. the system of the polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch as described in claim 1 to 8 is arbitrary adds
Preparation Method, it is characterised in that comprise the following steps:
(1) under normal temperature condition, boron nitride nanosheet, nano-silicon nitride are respectively classified into 2-4 equal portions, add the most by several times
In adhesive, stir, be placed in Vltrasonic device, supersound process 30-50min under 600W, obtain boron nitride nanosheet,
Nano-silicon nitride adhesive；
(2) being joined by polyamide in the prepared boron nitride nanosheet of step (1), nano-silicon nitride adhesive, stirring is all
Even so that be mixed with boron nitride nanosheet, the adhesive of nano-silicon nitride is uniformly dispersed in polyamide surface, is wrapped up
There are boron nitride nanosheet, the resin of nano-silicon nitride adhesive；
(3) under normal temperature condition, boron nitride powder being divided into 2-3 equal portions, join that step (2) prepares by several times is enclosed with nitridation
Boron nanometer sheet, nano-silicon nitride adhesive resin in, be uniformly mixed, then at 50-80 DEG C be dried 15-30h, obtain
Modified polyamide resin；
(4) polyamide and the metering conveying of nigrosine toner, metering and conveying device comprises two independent feed supplement feed bins and two
The weighing balance of platform band feed hopper, puts into respective feed supplement feed bin, then by mending by polyamide and nigrosine toner
Material feed bin enters the feed hopper on respective weighing balance, is finally delivered in double screw extruder melt extrude pelletize, tie rod water
Cold palletizing or underwater cutpellet, be dried 2-5h, obtain Organic Black Masterbatch at 80-120 DEG C after pelletize；
(5) modified polyamide resin step (3) prepared and step (4) join after preparing Organic Black Masterbatch mix homogeneously
In high-speed mixer, in high-speed mixer, then it is sequentially added into carbon fiber, maleic anhydride inoculated polypropylene wax, silane coupled
Agent, antioxidant, mix 20-40min, obtain compound under the mixing speed of 700-800r/min；
(6) compound that step (5) prepares is joined in double screw extruder, melt extrude pelletize, obtain after granulated and dried
The polyamide compoiste material that high heat conduction Organic Black Masterbatch adds.
The preparation method of the polyamide compoiste material that a kind of high heat conduction Organic Black Masterbatch the most as claimed in claim 9 adds,
It is characterized in that, when melt extruding pelletize in step (4), the screw zones of described double screw extruder and head temperature are respectively
For: feeding section: 115-125 DEG C, 200-220 DEG C, transportation section, melt zone 230-245 DEG C, head 225-230 DEG C.
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Denomination of invention: Polyamide composite material with high thermal conductivity organic black masterbatch addition and its preparation method Effective date of registration: 20231009 Granted publication date: 20180803 Pledgee: Bank of China Limited Shangyu sub branch Pledgor: ZHEJIANG JAVA SPECIALTY CHEMICALS Co.,Ltd. Registration number: Y2023980060206 |